zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2024-90-10-5-14zldm-2308Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISУстранение эффекта памяти для корректного определения ртути методом масс-спектрометрии с индуктивно-связанной плазмойEliminating the «memory effect» during mass spectrometric determination of mercuryЩукинВ. М.ShchukinV. M.

Виктор Михайлович Щукин

127051, Москва, Петровский бульвар, д. 8, стр. 2

Viktor M. Shchukin

8, bld. 2, Petrovsky bul., Moscow

schukin@expmed.ruКузьминаН. Е.Kuz’minaN. E.

Наталия Евгеньевна Кузьмина

127051, Москва, Петровский бульвар, д. 8, стр. 2

Natalia E. Kuz’mina

8, bld. 2, Petrovsky bul., Moscow

ЕринаА. А.ErinaA. A.

Алина Андреевна Ерина

127051, Москва, Петровский бульвар, д. 8, стр. 2

Alina A. Erina

8, bld. 2, Petrovsky bul., Moscow

БунятянН. Д.BunyatyanN. D.

Наталия Дмитриевна Бунятян

127051, Москва, Петровский бульвар, д. 8, стр. 2

Natalia D. Bunyatyan

8, bld. 2, Petrovsky bul., Moscow

Научный центр экспертизы средств медицинского применения Минздрава РоссииРоссияScientific Centre for Expert Evaluation of Medicinal ProductsRussian Federation2024221020249010514Copyright © Щукин В.М., Кузьмина Н.Е., Ерина А.А., Бунятян Н.Д., 20242024Щукин В.М., Кузьмина Н.Е., Ерина А.А., Бунятян Н.Д.Shchukin V.M., Kuz’mina N.E., Erina A.A., Bunyatyan N.D.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.zldm.ru/jour/article/view/2308

При определении ртути методом масс-спектрометрии с индуктивно-связанной плазмой (ИСП-МС) происходит адсорбция этого элемента на поверхности системы ввода проб прибора: эффект памяти искажает результаты определения следовых количеств ртути. Проведено экспериментальное сравнение эффективности предлагаемых в литературе способов удаления следовых количеств ртути для ее корректного определения методом ИСП-МС и выбран оптимальный отмывающий агент. В качестве отмывающих агентов для очистки системы ввода проб масс-спектрометра Agilent 7900 использовали разбавленные растворы азотной и соляной кислот, растворы хлорида золота, дихромата калия, тиомочевины, L-цистеина, бромида калия, бромата калия различных концентраций в воде, 1 %-ных азотной и соляной кислотах, а также водный раствор аммония пирролидиндитиокарбамата. Установлено, что фонового уровня содержания ртути удается достичь при использовании растворов хлорида золота (5 %), тиомочевины (0,01, 0,1 и 0,5 %), L-цистеина (2 %), бромида и бромата калия (0,5 ммоль/л) в 1,0 %-ной соляной кислоте. Фон понижается при использовании 3- и 5 %-ной HCl, растворов дихромата калия (60 мг/л), бромида и бромата калия (0,01 и 0,05 моль/л) в 1 %-ной соляной кислоте. Применение водного раствора аммония пирролидиндитиокарбамата вызывает резкую деградацию пластиковых трубок системы ввода проб. Эффективность отмывающих агентов на основе соляной кислоты выше, чем на основе азотной кислоты и воды. Наиболее перспективными отмывающими агентами являются бромсодержащие растворы и раствор бихромата калия в соляной кислоте. Оптимальным способом очистки прибора представляется его промывка 0,5 мМ раствором бромида калия в 1,0 %-ной соляной кислоте, что позволяет снизить интенсивность фонового сигнала изотопа 202Hg и не затрудняет определение других элементов.

When estimating mercury content by inductively coupled plasma mass spectrometry (ICP-MS), this element adsorbs on the surface of the sample introduction system of the instrument, which creates problems in the determination of trace amounts of mercury. Various methods of cleaning the instrument have been proposed in the literature. Objective: to experimentally compare the effectiveness of trace mercury removal methods proposed in the literature for elemental analysis by ICP-MS and to select the optimal cleaning agent. Methods: Mercury content in solution was determined by the Agilent Technologies 7900 inductively coupled plasma mass spectrometer using 202Hg isotope. Diluted solutions of nitric and hydrochloric acids, solutions of gold chloride, potassium dichromate, thiourea, L-cysteine, potassium bromide, potassium bromate of different concentrations in water and 1% nitric and hydrochloric acids, aqueous solution of ammonium pyrrolidinedithiocarbomate were used as washing agents. Results: The background level of mercury content is achieved by using solutions of copper chloride (5%), thiourea (0.01, 0.1, and 0.5%), L-cysteine (2%), potassium bromide and bromate (0.0005 M) in 1.0% hydrochloric acid solution. The background is lowered by using 3 and 5% HCl, potassium dichromate (60 mg/liter), potassium bromide and bromate (0.01 and 0.05 M) solutions in 1% hydrochloric acid. Application of aqueous solution of ammonium pyrrolidinedithiocarbamate causes sharp degradation of plastic tubes of the sample introduction system. Conclusion: The efficiency of washing agents based on hydrochloric acid is higher than that based on nitric acid and water. The most promising washing agents are bromide-containing solutions and potassium bichromate solution in hydrochloric acid. The optimal way to clean the device is its washing with 0.5 mM potassium bromide solution in 1.0% hydrochloric acid. Its use allows to reduce the background content of mercury and does not complicate the analysis of the content of other elements.

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The authors declare that there are no conflicts of interest present.